تفاعل #81798

معادلة التفاعل

hexane

Ethylamine

2-chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide

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title compound

المردود 76.2%

N-(2-Chloro-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide

المردود 76.2%

المذيبات

xylene

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvent was removed in vacuo and water
2. 2
   workup.ADDITIONadded to the residue
3. 3
   استخلاصThe product was extracted with ether
4. 4
   تجفيفdried (sodium sulfate)
5. 5
   تركيزconcentrated
6. 6
   أخرىto give an oil
7. 7
   أخرىformed
8. 8
   ترشيحThe solid was filtered
9. 9
   أخرىdried

الإجراء التجريبي

Ethylamine (12.7 g) was added to a suspension of 21.0 g of the 2-chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide in 150 ml of xylene in a steel bomb. The mixture was then heated in an oil bath to 165° C. for 6 hrs. and then stirred overnight at room temperature. The solvent was removed in vacuo and water added to the residue. The product was extracted with ether, dried (sodium sulfate) and concentrated to give an oil. This was dissolved in ethyl acetate followed by hexane at which time a precipitate formed. The solid was filtered and dried to give 16.5 g of the title compound, m.p. 122°-124° C.

المصدر